# Electronic Supplementary Material (ESI) for Chemical Communications
# This journal is © The Royal Society of Chemistry 2013


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# 
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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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#  fide research purposes only. It may contain copyright material 
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data_fgadfl
_database_code_depnum_ccdc_archive 'CCDC 822015'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Phenyl-Glycyl-Alanyl-(\a,\b-dehydrophenylalanyl)-Leucine dihydrate'
_chemical_name_common            'PEPSEQ A=5 PHE-GLY-ALA-PHE*-LEU'
_chemical_formula_moiety         'C29 H37 N5 O6, 2(H2 O1)'
_chemical_formula_sum            'C29 H41 N5 O8'
_exptl_crystal_recrystallization_method 
'0.02M CaCl2.2(H2O); 0.1M Sodium acetate trihydrate; pH 4.6; MPD 30 % ( v/v)'
_chemical_melting_point          ?
_exptl_crystal_description       ?
_exptl_crystal_colour            Colourless
_diffrn_ambient_temperature      100
_chemical_formula_weight         551.64
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P 21 21 21'
_symmetry_int_tables_number      19
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
_cell_length_a                   8.9951(9)
_cell_length_b                   13.0144(12)
_cell_length_c                   27.752(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3248.8(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.128
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1176
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD detector'
_diffrn_measurement_method       '\w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            59104
_diffrn_reflns_av_R_equivalents  0.1140
_diffrn_reflns_av_sigmaI/netI    0.0674
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.47
_diffrn_reflns_theta_max         23.34
_reflns_number_total             4703
_reflns_number_gt                2581
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'KAPPA APEX II (BRUKER-AXS)'
_computing_cell_refinement       'SAINTPLUS (BRUKER-AXS)'
_computing_data_reduction        'SAINTPLUS (BRUKER-AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0984P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0071(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   1(2)
_refine_ls_number_reflns         4703
_refine_ls_number_parameters     377
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1356
_refine_ls_R_factor_gt           0.0595
_refine_ls_wR_factor_ref         0.1825
_refine_ls_wR_factor_gt          0.1400
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.033
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C5B C 0.1187(15) 0.0788(8) 0.0876(3) 0.063(4) Uiso 0.531(11) 1 d PD A 1
H5B1 H 0.0341 0.1236 0.0822 0.076 Uiso 0.531(11) 1 calc PR A 1
H5B2 H 0.2087 0.1195 0.0851 0.076 Uiso 0.531(11) 1 calc PR A 1
C5G C 0.1082(12) 0.0295(7) 0.1381(3) 0.065(3) Uiso 0.531(11) 1 d PD A 1
H5G H 0.0273 -0.0209 0.1380 0.078 Uiso 0.531(11) 1 calc PR A 1
C5D1 C 0.2505(17) -0.0241(12) 0.1516(6) 0.110(5) Uiso 0.531(11) 1 d PD A 1
H5D1 H 0.2395 -0.0555 0.1827 0.165 Uiso 0.531(11) 1 calc PR A 1
H5D2 H 0.3302 0.0249 0.1526 0.165 Uiso 0.531(11) 1 calc PR A 1
H5D3 H 0.2727 -0.0760 0.1281 0.165 Uiso 0.531(11) 1 calc PR A 1
C5D2 C 0.0726(19) 0.1130(11) 0.1750(5) 0.124(5) Uiso 0.531(11) 1 d PD A 1
H5D4 H -0.0189 0.1462 0.1664 0.186 Uiso 0.531(11) 1 calc PR A 1
H5D5 H 0.1514 0.1627 0.1755 0.186 Uiso 0.531(11) 1 calc PR A 1
H5D6 H 0.0630 0.0825 0.2064 0.186 Uiso 0.531(11) 1 calc PR A 1
C5B' C 0.0723(12) 0.0505(9) 0.0992(4) 0.048(3) Uiso 0.469(11) 1 d PD A 2
H5B3 H 0.0031 0.1052 0.0914 0.058 Uiso 0.469(11) 1 calc PR A 2
H5B4 H 0.0209 0.0018 0.1198 0.058 Uiso 0.469(11) 1 calc PR A 2
C5G' C 0.2025(13) 0.0955(8) 0.1268(4) 0.070(4) Uiso 0.469(11) 1 d PD A 2
H5G' H 0.2589 0.1385 0.1043 0.084 Uiso 0.469(11) 1 calc PR A 2
C5D' C 0.3068(16) 0.0161(11) 0.1463(5) 0.075(4) Uiso 0.469(11) 1 d PD A 2
H5D7 H 0.3865 0.0494 0.1632 0.113 Uiso 0.469(11) 1 calc PR A 2
H5D8 H 0.3467 -0.0237 0.1202 0.113 Uiso 0.469(11) 1 calc PR A 2
H5D9 H 0.2542 -0.0283 0.1680 0.113 Uiso 0.469(11) 1 calc PR A 2
C5D" C 0.1472(16) 0.1654(10) 0.1676(4) 0.079(4) Uiso 0.469(11) 1 d PD A 2
H5DX H 0.2309 0.1941 0.1843 0.118 Uiso 0.469(11) 1 calc PR A 2
H5DY H 0.0881 0.1259 0.1897 0.118 Uiso 0.469(11) 1 calc PR A 2
H5DZ H 0.0881 0.2198 0.1543 0.118 Uiso 0.469(11) 1 calc PR A 2
N1 N 0.2776(5) 0.7205(3) 0.03529(14) 0.0624(11) Uani 1 1 d . . .
H1A H 0.3386 0.7742 0.0371 0.094 Uiso 1 1 calc R . .
H1B H 0.1844 0.7414 0.0397 0.094 Uiso 1 1 calc R . .
H1C H 0.2860 0.6913 0.0064 0.094 Uiso 1 1 calc R . .
C1A C 0.3176(6) 0.6445(3) 0.07323(16) 0.0547(13) Uani 1 1 d D . .
H1A1 H 0.4199 0.6206 0.0685 0.066 Uiso 1 1 calc R . .
C1' C 0.2098(7) 0.5559(4) 0.06730(17) 0.0573(13) Uani 1 1 d . . .
O1' O 0.0786(5) 0.5723(2) 0.05789(15) 0.0805(12) Uani 1 1 d . . .
C1B C 0.3025(7) 0.6965(4) 0.12225(17) 0.0723(16) Uani 1 1 d D . .
H1B1 H 0.3499 0.7634 0.1209 0.087 Uiso 1 1 calc R . .
H1B2 H 0.1979 0.7073 0.1291 0.087 Uiso 1 1 calc R . .
C1G C 0.3704(8) 0.6355(5) 0.1628(2) 0.0845(18) Uani 1 1 d D . .
C1D1 C 0.2976(11) 0.5562(6) 0.1844(3) 0.139(3) Uani 1 1 d D . .
H1D1 H 0.2025 0.5406 0.1735 0.167 Uiso 1 1 calc R . .
C1D2 C 0.5105(10) 0.6548(8) 0.1794(3) 0.138(3) Uani 1 1 d D . .
H1D2 H 0.5662 0.7066 0.1650 0.166 Uiso 1 1 calc R . .
C1E1 C 0.3552(18) 0.4972(9) 0.2213(4) 0.212(7) Uani 1 1 d D . .
H1E1 H 0.3008 0.4442 0.2354 0.254 Uiso 1 1 calc R . .
C1E2 C 0.5728(16) 0.5986(12) 0.2176(4) 0.214(9) Uani 1 1 d D . .
H1E2 H 0.6661 0.6151 0.2298 0.257 Uiso 1 1 calc R . .
C1Z C 0.494(2) 0.5202(12) 0.2360(6) 0.244(13) Uani 1 1 d D . .
H1Z H 0.5371 0.4800 0.2599 0.293 Uiso 1 1 calc R . .
N2 N 0.2609(4) 0.4607(3) 0.07376(13) 0.0556(10) Uani 1 1 d . . .
H2 H 0.3542 0.4509 0.0788 0.067 Uiso 1 1 calc R . .
C2A C 0.1609(6) 0.3736(4) 0.0724(2) 0.0679(15) Uani 1 1 d . . .
H2A1 H 0.0762 0.3892 0.0928 0.081 Uiso 1 1 calc R . .
H2A2 H 0.2117 0.3152 0.0866 0.081 Uiso 1 1 calc R . .
C2' C 0.1035(6) 0.3416(3) 0.0244(2) 0.0598(14) Uani 1 1 d . . .
O2' O 0.0016(4) 0.2774(3) 0.02281(15) 0.0785(11) Uani 1 1 d . . .
N3 N 0.1617(5) 0.3804(3) -0.01557(16) 0.0595(12) Uani 1 1 d . . .
H3 H 0.2415 0.4167 -0.0146 0.071 Uiso 1 1 calc R . .
C3A C 0.0869(6) 0.3598(4) -0.0614(2) 0.0649(15) Uani 1 1 d . . .
H3A H -0.0157 0.3846 -0.0589 0.078 Uiso 1 1 calc R . .
C3' C 0.0819(7) 0.2467(4) -0.0731(2) 0.0659(15) Uani 1 1 d . . .
O3' O -0.0298(5) 0.2080(3) -0.09143(16) 0.0922(13) Uani 1 1 d . . .
C3B C 0.1621(7) 0.4176(4) -0.1023(2) 0.0824(18) Uani 1 1 d . . .
H3B1 H 0.1638 0.4897 -0.0950 0.124 Uiso 1 1 calc R . .
H3B2 H 0.1078 0.4066 -0.1317 0.124 Uiso 1 1 calc R . .
H3B3 H 0.2620 0.3930 -0.1061 0.124 Uiso 1 1 calc R . .
N4 N 0.2058(5) 0.1924(3) -0.06542(15) 0.0635(11) Uani 1 1 d . . .
H4 H 0.2832 0.2238 -0.0547 0.076 Uiso 1 1 calc R . .
C4A C 0.2153(6) 0.0837(4) -0.0742(2) 0.0692(16) Uani 1 1 d D . .
C4' C 0.1867(6) 0.0130(4) -0.0328(2) 0.0654(15) Uani 1 1 d . . .
O4' O 0.1978(4) -0.0807(3) -0.03651(14) 0.0819(12) Uani 1 1 d . . .
C4B C 0.2576(7) 0.0437(5) -0.1168(2) 0.0843(18) Uani 1 1 d D . .
H4B H 0.2638 -0.0276 -0.1179 0.101 Uiso 1 1 calc R . .
C4G C 0.2955(8) 0.0977(6) -0.1620(3) 0.099(2) Uani 1 1 d D . .
C4D1 C 0.2218(10) 0.1840(6) -0.1793(3) 0.122(3) Uani 1 1 d D . .
H4D1 H 0.1437 0.2128 -0.1620 0.146 Uiso 1 1 calc R . .
C4D2 C 0.4086(10) 0.0589(7) -0.1891(3) 0.146(3) Uani 1 1 d D . .
H4D2 H 0.4585 0.0010 -0.1779 0.175 Uiso 1 1 calc R . .
C4E1 C 0.2663(14) 0.2270(7) -0.2232(4) 0.155(4) Uani 1 1 d D . .
H4E1 H 0.2173 0.2846 -0.2350 0.186 Uiso 1 1 calc R . .
C4E2 C 0.4529(13) 0.1020(11) -0.2328(4) 0.195(6) Uani 1 1 d D . .
H4E2 H 0.5307 0.0735 -0.2503 0.234 Uiso 1 1 calc R . .
C4Z C 0.3812(15) 0.1852(11) -0.2488(4) 0.193(6) Uani 1 1 d D . .
H4Z H 0.4099 0.2152 -0.2778 0.231 Uiso 1 1 calc R . .
N5 N 0.1471(5) 0.0568(3) 0.00816(17) 0.0639(12) Uani 1 1 d . A .
H5 H 0.1371 0.1225 0.0097 0.077 Uiso 1 1 calc R . .
C5A C 0.1203(6) -0.0060(4) 0.05066(19) 0.0661(15) Uani 1 1 d D . .
H5A H 0.2098 -0.0473 0.0563 0.079 Uiso 1 1 calc R A 1
C5' C -0.0088(7) -0.0800(4) 0.04363(18) 0.0613(14) Uani 1 1 d . A .
O5' O -0.1248(4) -0.0478(2) 0.02437(13) 0.0662(9) Uani 1 1 d . . .
O5" O 0.0099(4) -0.1706(3) 0.05870(14) 0.0804(12) Uani 1 1 d . . .
O1W O 0.7258(5) 0.7657(3) 0.08176(15) 0.0970(13) Uani 1 1 d . . .
O2W O 0.4928(4) 0.8732(3) 0.04041(14) 0.0868(12) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.061(3) 0.057(2) 0.069(3) 0.003(2) 0.003(2) -0.007(2)
C1A 0.065(4) 0.041(3) 0.058(3) 0.001(2) -0.002(3) 0.005(2)
C1' 0.058(4) 0.048(3) 0.066(3) 0.008(2) 0.005(3) 0.009(3)
O1' 0.055(3) 0.059(2) 0.128(3) 0.018(2) -0.004(2) 0.0071(19)
C1B 0.090(5) 0.062(3) 0.064(3) -0.008(3) -0.002(3) 0.005(3)
C1G 0.087(5) 0.104(5) 0.063(4) -0.023(4) -0.001(4) -0.001(4)
C1D1 0.182(10) 0.140(7) 0.094(6) 0.031(5) -0.025(6) -0.022(7)
C1D2 0.102(7) 0.235(10) 0.078(5) -0.042(6) -0.001(5) 0.013(7)
C1E1 0.36(2) 0.161(10) 0.120(9) 0.055(7) -0.052(11) -0.002(13)
C1E2 0.178(13) 0.36(3) 0.101(10) -0.088(13) -0.066(9) 0.111(15)
C1Z 0.35(3) 0.235(19) 0.149(15) -0.064(12) -0.074(16) 0.16(2)
N2 0.050(3) 0.049(2) 0.068(3) 0.004(2) 0.006(2) 0.000(2)
C2A 0.065(4) 0.051(3) 0.087(4) 0.011(3) 0.021(3) 0.003(3)
C2' 0.056(4) 0.035(3) 0.089(4) 0.003(3) 0.014(3) 0.001(3)
O2' 0.064(3) 0.051(2) 0.120(3) -0.006(2) 0.023(2) -0.013(2)
N3 0.050(3) 0.052(2) 0.076(3) 0.004(2) 0.003(2) -0.015(2)
C3A 0.053(3) 0.053(3) 0.089(4) 0.004(3) -0.011(3) -0.002(3)
C3' 0.052(4) 0.057(3) 0.090(4) -0.001(3) -0.007(3) -0.008(3)
O3' 0.062(3) 0.074(2) 0.140(4) -0.011(3) -0.025(3) -0.013(2)
C3B 0.101(5) 0.064(3) 0.082(4) 0.004(3) -0.012(4) -0.012(3)
N4 0.048(3) 0.050(3) 0.093(3) -0.003(2) -0.010(2) -0.007(2)
C4A 0.052(4) 0.057(3) 0.099(5) -0.017(3) -0.016(3) -0.001(3)
C4' 0.059(4) 0.044(3) 0.093(5) 0.000(3) 0.000(3) -0.005(2)
O4' 0.097(3) 0.044(2) 0.105(3) -0.0135(19) 0.006(2) 0.0030(19)
C4B 0.088(5) 0.073(4) 0.092(5) -0.016(4) -0.012(4) 0.000(4)
C4G 0.098(6) 0.113(6) 0.086(5) -0.030(5) -0.012(5) -0.016(5)
C4D1 0.174(9) 0.110(6) 0.082(5) -0.009(5) -0.019(5) 0.006(6)
C4D2 0.120(8) 0.225(10) 0.093(6) -0.013(7) -0.006(6) 0.007(7)
C4E1 0.211(13) 0.155(8) 0.099(8) 0.019(6) -0.042(7) -0.031(9)
C4E2 0.132(11) 0.36(2) 0.096(9) -0.008(10) -0.001(7) -0.017(11)
C4Z 0.180(15) 0.31(2) 0.089(8) 0.000(10) -0.012(9) -0.061(14)
N5 0.069(3) 0.039(2) 0.084(3) -0.010(2) -0.003(2) 0.000(2)
C5A 0.064(4) 0.054(3) 0.080(4) -0.008(3) -0.020(3) 0.019(3)
C5' 0.065(4) 0.059(3) 0.060(3) -0.002(3) 0.001(3) 0.011(3)
O5' 0.067(2) 0.0502(19) 0.082(2) 0.0013(18) -0.013(2) 0.0098(18)
O5" 0.084(3) 0.058(2) 0.099(3) 0.025(2) -0.007(2) 0.011(2)
O1W 0.106(3) 0.075(3) 0.111(3) -0.015(2) 0.016(3) -0.005(2)
O2W 0.079(3) 0.071(2) 0.110(3) -0.014(2) 0.018(2) -0.014(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C5B C5A 1.506(9) . ?
C5B C5G 1.544(13) . ?
C5G C5D1 1.505(13) . ?
C5G C5D2 1.528(13) . ?
C5B' C5G' 1.516(13) . ?
C5B' C5A 1.596(10) . ?
C5G' C5D' 1.497(13) . ?
C5G' C5D" 1.535(13) . ?
N1 C1A 1.488(6) . ?
C1A C1' 1.516(7) . ?
C1A C1B 1.526(6) . ?
C1' O1' 1.228(6) . ?
C1' N2 1.334(6) . ?
C1B C1G 1.506(8) . ?
C1G C1D1 1.361(9) . ?
C1G C1D2 1.365(9) . ?
C1D1 C1E1 1.382(11) . ?
C1D2 C1E2 1.405(12) . ?
C1E1 C1Z 1.346(15) . ?
C1E2 C1Z 1.344(15) . ?
N2 C2A 1.448(6) . ?
C2A C2' 1.489(8) . ?
C2' O2' 1.241(6) . ?
C2' N3 1.326(6) . ?
N3 C3A 1.464(6) . ?
C3A C3' 1.508(7) . ?
C3A C3B 1.521(7) . ?
C3' O3' 1.233(6) . ?
C3' N4 1.338(7) . ?
N4 C4A 1.438(6) . ?
C4A C4B 1.345(7) . ?
C4A C4' 1.494(8) . ?
C4' O4' 1.228(5) . ?
C4' N5 1.322(6) . ?
C4B C4G 1.478(9) . ?
C4G C4D2 1.362(9) . ?
C4G C4D1 1.391(9) . ?
C4D1 C4E1 1.397(10) . ?
C4D2 C4E2 1.394(11) . ?
C4E1 C4Z 1.367(12) . ?
C4E2 C4Z 1.337(13) . ?
N5 C5A 1.456(6) . ?
C5A C5' 1.521(7) . ?
C5' O5' 1.245(6) . ?
C5' O5" 1.262(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C5A C5B C5G 108.2(8) . . ?
C5D1 C5G C5D2 109.9(11) . . ?
C5D1 C5G C5B 111.6(10) . . ?
C5D2 C5G C5B 109.0(8) . . ?
C5G' C5B' C5A 113.3(8) . . ?
C5D' C5G' C5B' 113.6(10) . . ?
C5D' C5G' C5D" 110.2(10) . . ?
C5B' C5G' C5D" 110.5(9) . . ?
N1 C1A C1' 105.9(4) . . ?
N1 C1A C1B 108.3(4) . . ?
C1' C1A C1B 112.2(4) . . ?
O1' C1' N2 121.4(5) . . ?
O1' C1' C1A 120.4(4) . . ?
N2 C1' C1A 118.2(5) . . ?
C1G C1B C1A 113.3(4) . . ?
C1D1 C1G C1D2 115.8(7) . . ?
C1D1 C1G C1B 122.3(7) . . ?
C1D2 C1G C1B 121.9(7) . . ?
C1G C1D1 C1E1 124.6(10) . . ?
C1G C1D2 C1E2 121.8(10) . . ?
C1Z C1E1 C1D1 116.6(13) . . ?
C1Z C1E2 C1D2 118.2(14) . . ?
C1E2 C1Z C1E1 122.9(17) . . ?
C1' N2 C2A 120.6(4) . . ?
N2 C2A C2' 117.2(4) . . ?
O2' C2' N3 121.2(5) . . ?
O2' C2' C2A 118.4(5) . . ?
N3 C2' C2A 120.4(5) . . ?
C2' N3 C3A 118.4(4) . . ?
N3 C3A C3' 112.3(4) . . ?
N3 C3A C3B 110.7(4) . . ?
C3' C3A C3B 109.6(5) . . ?
O3' C3' N4 121.9(5) . . ?
O3' C3' C3A 120.8(5) . . ?
N4 C3' C3A 117.2(5) . . ?
C3' N4 C4A 122.9(4) . . ?
C4B C4A N4 123.1(5) . . ?
C4B C4A C4' 119.0(5) . . ?
N4 C4A C4' 117.7(5) . . ?
O4' C4' N5 121.5(5) . . ?
O4' C4' C4A 122.3(6) . . ?
N5 C4' C4A 116.2(5) . . ?
C4A C4B C4G 128.7(6) . . ?
C4D2 C4G C4D1 117.6(8) . . ?
C4D2 C4G C4B 117.7(8) . . ?
C4D1 C4G C4B 124.7(7) . . ?
C4G C4D1 C4E1 119.3(8) . . ?
C4G C4D2 C4E2 123.0(10) . . ?
C4Z C4E1 C4D1 120.7(11) . . ?
C4Z C4E2 C4D2 118.5(12) . . ?
C4E2 C4Z C4E1 120.9(13) . . ?
C4' N5 C5A 119.9(4) . . ?
N5 C5A C5B 98.1(5) . . ?
N5 C5A C5' 112.2(4) . . ?
C5B C5A C5' 122.9(7) . . ?
N5 C5A C5B' 118.0(6) . . ?
C5B C5A C5B' 23.7(5) . . ?
C5' C5A C5B' 101.2(6) . . ?
O5' C5' O5" 124.7(5) . . ?
O5' C5' C5A 118.8(5) . . ?
O5" C5' C5A 116.5(5) . . ?
_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        23.34
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.381
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.110


data_fgadfi
_database_code_depnum_ccdc_archive 'CCDC 904790'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
'Phenyl-Glycyl-Alanyl-(\a,\b-dehydrophenylalanyl)-Isoleucine dihydrate'
_chemical_name_common            'PEPSEQ A=5 PHE-GLY-ALA-PHE*-ILE'
_chemical_formula_moiety         'C29 H37 N5 O6, 2(H2 O1)'
_chemical_formula_sum            'C29 H41 N5 O8'
_exptl_crystal_recrystallization_method 
'0.2 M Ammonium sulphate; 0.1M Sodium cacodylate trihydrate; pH 6.5; PEG 8000-30%(w/v) '
_chemical_melting_point          ?
_exptl_crystal_description       ?
_exptl_crystal_colour            Colourless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         551.64
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21'
_symmetry_int_tables_number      4
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z'
_cell_length_a                   12.895(2)
_cell_length_b                   9.0534(16)
_cell_length_c                   13.089(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.071(9)
_cell_angle_gamma                90.00
_cell_volume                     1482.2(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.01
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             628
_exptl_absorpt_coefficient_mu    0.097
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.9809
_exptl_absorpt_correction_T_max  0.9990
_exptl_absorpt_process_details   ?
_exptl_special_details           
;
?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker Kappa APEX II CCD detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            11784
_diffrn_reflns_av_R_equivalents  0.1060
_diffrn_reflns_av_sigmaI/netI    0.1231
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         1.63
_diffrn_reflns_theta_max         24.51
_reflns_number_total             4024
_reflns_number_gt                2612
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'KAPPA APEX II (BRUKER-AXS)'
_computing_cell_refinement       'SAINTPLUS (BRUKER-AXS)'
_computing_data_reduction        'SAINTPLUS (BRUKER-AXS)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0108(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.7(17)
_refine_ls_number_reflns         4024
_refine_ls_number_parameters     396
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1030
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1067
_refine_ls_wR_factor_gt          0.0892
_refine_ls_goodness_of_fit_ref   0.978
_refine_ls_restrained_S_all      0.978
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N1 N 0.5710(3) 0.5656(4) 0.4948(3) 0.0229(10) Uani 1 1 d . . .
H1A H 0.5744 0.6302 0.5488 0.034 Uiso 1 1 calc R . .
H1B H 0.5845 0.4726 0.5210 0.034 Uiso 1 1 calc R . .
H1C H 0.5045 0.5688 0.4507 0.034 Uiso 1 1 calc R . .
C1A C 0.6522(4) 0.6072(5) 0.4357(4) 0.0219(12) Uani 1 1 d . . .
H1A1 H 0.6376 0.7095 0.4071 0.026 Uiso 1 1 calc R . .
C1' C 0.6414(4) 0.4986(6) 0.3456(4) 0.0220(12) Uani 1 1 d . . .
O1' O 0.6234(3) 0.3689(4) 0.3579(3) 0.0271(9) Uani 1 1 d . . .
C1B C 0.7616(4) 0.6021(5) 0.5130(4) 0.0263(13) Uani 1 1 d . . .
H1B1 H 0.7639 0.6785 0.5676 0.032 Uiso 1 1 calc R . .
H1B2 H 0.7703 0.5048 0.5485 0.032 Uiso 1 1 calc R . .
C1G C 0.8552(4) 0.6265(5) 0.4635(4) 0.0257(13) Uani 1 1 d . . .
C1D1 C 0.8560(4) 0.7290(5) 0.3859(4) 0.0301(14) Uani 1 1 d . . .
H1D1 H 0.7952 0.7901 0.3607 0.036 Uiso 1 1 calc R . .
C1D2 C 0.9475(4) 0.5421(6) 0.5023(4) 0.0301(14) Uani 1 1 d . . .
H1D2 H 0.9484 0.4704 0.5555 0.036 Uiso 1 1 calc R . .
C1E1 C 0.9453(4) 0.7440(6) 0.3438(4) 0.0344(14) Uani 1 1 d . . .
H1E1 H 0.9433 0.8108 0.2874 0.041 Uiso 1 1 calc R . .
C1E2 C 1.0382(4) 0.5627(6) 0.4632(4) 0.0329(14) Uani 1 1 d . . .
H1E2 H 1.1013 0.5076 0.4917 0.039 Uiso 1 1 calc R . .
C1Z C 1.0360(5) 0.6625(6) 0.3838(4) 0.0362(15) Uani 1 1 d . . .
H1Z H 1.0972 0.6753 0.3564 0.043 Uiso 1 1 calc R . .
N2 N 0.6534(3) 0.5532(4) 0.2548(3) 0.0191(10) Uani 1 1 d . . .
H2 H 0.6574 0.6494 0.2471 0.023 Uiso 1 1 calc R . .
C2A C 0.6598(4) 0.4564(5) 0.1683(4) 0.0231(12) Uani 1 1 d . . .
H2A1 H 0.7062 0.3717 0.1975 0.028 Uiso 1 1 calc R . .
H2A2 H 0.6956 0.5109 0.1210 0.028 Uiso 1 1 calc R . .
C2' C 0.5568(4) 0.3970(5) 0.1037(4) 0.0188(12) Uani 1 1 d . . .
O2' O 0.5590(2) 0.3023(3) 0.0360(2) 0.0226(8) Uani 1 1 d . . .
N3 N 0.4635(3) 0.4448(4) 0.1199(3) 0.0213(10) Uani 1 1 d . . .
H3 H 0.4608 0.5205 0.1613 0.026 Uiso 1 1 calc R . .
C3A C 0.3669(4) 0.3663(5) 0.0661(4) 0.0213(12) Uani 1 1 d . . .
H3A H 0.3766 0.2600 0.0870 0.026 Uiso 1 1 calc R . .
C3' C 0.3480(4) 0.3736(5) -0.0521(4) 0.0210(12) Uani 1 1 d . . .
O3' O 0.3075(3) 0.2698(4) -0.1075(3) 0.0291(9) Uani 1 1 d . . .
C3B C 0.2704(4) 0.4238(6) 0.1019(4) 0.0276(13) Uani 1 1 d . . .
H3B1 H 0.2846 0.4176 0.1788 0.041 Uiso 1 1 calc R . .
H3B2 H 0.2075 0.3639 0.0701 0.041 Uiso 1 1 calc R . .
H3B3 H 0.2569 0.5269 0.0799 0.041 Uiso 1 1 calc R . .
N4 N 0.3717(3) 0.5001(4) -0.0941(3) 0.0196(9) Uani 1 1 d . . .
H4 H 0.3989 0.5731 -0.0516 0.023 Uiso 1 1 calc R . .
C4A C 0.3548(4) 0.5216(5) -0.2050(4) 0.0185(11) Uani 1 1 d . . .
C4' C 0.4458(4) 0.4793(5) -0.2530(4) 0.0200(12) Uani 1 1 d . . .
O4' O 0.4384(3) 0.4914(4) -0.3486(2) 0.0281(9) Uani 1 1 d . . .
C4B C 0.2679(4) 0.5791(5) -0.2665(4) 0.0219(12) Uani 1 1 d . . .
H4B H 0.2702 0.5936 -0.3378 0.026 Uiso 1 1 calc R . .
C4G C 0.1671(4) 0.6242(5) -0.2401(4) 0.0221(12) Uani 1 1 d . . .
C4D1 C 0.1273(4) 0.5554(6) -0.1630(4) 0.0289(14) Uani 1 1 d . . .
H4D1 H 0.1666 0.4779 -0.1223 0.035 Uiso 1 1 calc R . .
C4D2 C 0.1074(4) 0.7382(6) -0.2978(4) 0.0282(13) Uani 1 1 d . . .
H4D2 H 0.1331 0.7863 -0.3513 0.034 Uiso 1 1 calc R . .
C4E1 C 0.0305(4) 0.5996(6) -0.1452(4) 0.0337(14) Uani 1 1 d . . .
H4E1 H 0.0036 0.5517 -0.0925 0.040 Uiso 1 1 calc R . .
C4E2 C 0.0117(4) 0.7821(6) -0.2784(4) 0.0329(14) Uani 1 1 d . . .
H4E2 H -0.0275 0.8611 -0.3175 0.040 Uiso 1 1 calc R . .
C4Z C -0.0268(4) 0.7115(6) -0.2029(4) 0.0327(14) Uani 1 1 d . . .
H4Z H -0.0934 0.7404 -0.1904 0.039 Uiso 1 1 calc R . .
N5 N 0.5355(3) 0.4301(4) -0.1876(3) 0.0216(10) Uani 1 1 d . . .
H5 H 0.5396 0.4201 -0.1199 0.026 Uiso 1 1 calc R . .
C5A C 0.6274(4) 0.3930(5) -0.2313(4) 0.0190(12) Uani 1 1 d . . .
H5A H 0.6460 0.4820 -0.2685 0.023 Uiso 1 1 calc R . .
C5' C 0.5994(4) 0.2658(6) -0.3114(4) 0.0214(12) Uani 1 1 d . . .
O5' O 0.5620(2) 0.1489(3) -0.2842(2) 0.0240(8) Uani 1 1 d . . .
C5B C 0.7241(4) 0.3532(5) -0.1420(4) 0.0222(12) Uani 1 1 d . . .
H5B H 0.7014 0.2755 -0.0977 0.027 Uiso 1 1 calc R . .
C5G1 C 0.7633(4) 0.4863(5) -0.0721(4) 0.0258(13) Uani 1 1 d . . .
H5G1 H 0.7898 0.5617 -0.1143 0.031 Uiso 1 1 calc R . .
H5G2 H 0.7020 0.5297 -0.0496 0.031 Uiso 1 1 calc R . .
C5G2 C 0.8134(4) 0.2884(6) -0.1874(4) 0.0308(13) Uani 1 1 d . . .
H5G3 H 0.7863 0.2021 -0.2309 0.046 Uiso 1 1 calc R . .
H5G4 H 0.8735 0.2587 -0.1296 0.046 Uiso 1 1 calc R . .
H5G5 H 0.8375 0.3631 -0.2307 0.046 Uiso 1 1 calc R . .
C5D C 0.8517(4) 0.4520(6) 0.0256(4) 0.0302(13) Uani 1 1 d . . .
H5D1 H 0.8728 0.5430 0.0658 0.045 Uiso 1 1 calc R . .
H5D2 H 0.9136 0.4109 0.0043 0.045 Uiso 1 1 calc R . .
H5D3 H 0.8256 0.3801 0.0694 0.045 Uiso 1 1 calc R . .
O5" O 0.6220(3) 0.2855(4) -0.3989(3) 0.0287(9) Uani 1 1 d . . .
O1W O 0.5947(4) 0.7798(4) 0.6493(3) 0.0319(10) Uani 1 1 d . . .
O2W O 0.6849(3) 0.0053(4) 0.5520(3) 0.0315(10) Uani 1 1 d . . .
H1W H 0.626(4) 0.862(6) 0.625(4) 0.029(15) Uiso 1 1 d . . .
H3W H 0.645(4) -0.002(5) 0.488(4) 0.029(17) Uiso 1 1 d . . .
H4W H 0.665(4) 0.099(6) 0.562(4) 0.042(18) Uiso 1 1 d . . .
H2W H 0.541(4) 0.796(7) 0.650(5) 0.04(2) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.027(2) 0.026(3) 0.018(2) 0.0026(19) 0.010(2) 0.0012(19)
C1A 0.027(3) 0.022(3) 0.019(3) 0.003(2) 0.011(2) 0.000(2)
C1' 0.026(3) 0.019(3) 0.023(3) 0.003(3) 0.009(2) 0.002(2)
O1' 0.043(2) 0.018(2) 0.027(2) 0.0005(17) 0.0206(18) -0.0012(17)
C1B 0.030(3) 0.032(3) 0.016(3) -0.002(2) 0.005(3) -0.004(2)
C1G 0.030(3) 0.028(3) 0.019(3) -0.007(3) 0.006(3) -0.001(3)
C1D1 0.030(3) 0.027(3) 0.033(4) -0.005(3) 0.007(3) -0.002(2)
C1D2 0.033(3) 0.032(4) 0.025(3) 0.003(3) 0.007(3) 0.000(3)
C1E1 0.041(4) 0.034(4) 0.027(3) 0.001(3) 0.006(3) -0.016(3)
C1E2 0.030(3) 0.036(4) 0.034(4) -0.006(3) 0.012(3) 0.004(3)
C1Z 0.045(4) 0.036(4) 0.032(4) -0.005(3) 0.018(3) -0.009(3)
N2 0.034(3) 0.013(2) 0.013(2) 0.0035(18) 0.0103(19) 0.0063(18)
C2A 0.032(3) 0.022(3) 0.018(3) -0.005(2) 0.011(2) -0.002(2)
C2' 0.034(3) 0.016(3) 0.008(3) 0.005(2) 0.009(2) 0.004(2)
O2' 0.037(2) 0.021(2) 0.0117(19) -0.0020(15) 0.0100(16) 0.0009(16)
N3 0.029(3) 0.022(2) 0.015(2) -0.0081(18) 0.0098(19) 0.001(2)
C3A 0.030(3) 0.018(3) 0.017(3) 0.001(2) 0.008(3) 0.002(2)
C3' 0.028(3) 0.012(3) 0.026(3) 0.000(3) 0.011(3) 0.001(2)
O3' 0.043(2) 0.022(2) 0.026(2) -0.0049(18) 0.0149(18) -0.0042(18)
C3B 0.038(3) 0.030(3) 0.018(3) -0.001(2) 0.012(2) 0.002(3)
N4 0.029(2) 0.016(2) 0.014(2) -0.0047(19) 0.0068(19) 0.0000(19)
C4A 0.033(3) 0.011(3) 0.014(3) 0.002(2) 0.010(2) -0.002(2)
C4' 0.026(3) 0.016(3) 0.019(3) 0.001(2) 0.007(3) -0.004(2)
O4' 0.039(2) 0.033(2) 0.014(2) 0.0025(17) 0.0086(16) 0.0017(17)
C4B 0.036(3) 0.017(3) 0.015(3) 0.000(2) 0.011(3) 0.002(2)
C4G 0.028(3) 0.020(3) 0.017(3) -0.003(2) 0.003(2) -0.002(2)
C4D1 0.032(3) 0.028(3) 0.029(4) 0.006(3) 0.011(3) 0.000(2)
C4D2 0.035(3) 0.030(3) 0.021(3) 0.001(3) 0.009(3) -0.002(3)
C4E1 0.037(4) 0.041(4) 0.027(3) -0.001(3) 0.016(3) -0.004(3)
C4E2 0.034(3) 0.032(3) 0.033(4) 0.003(3) 0.009(3) 0.004(3)
C4Z 0.028(3) 0.031(3) 0.042(4) -0.001(3) 0.013(3) 0.004(3)
N5 0.032(3) 0.025(2) 0.010(2) 0.0003(19) 0.009(2) 0.003(2)
C5A 0.026(3) 0.021(3) 0.013(3) 0.004(2) 0.010(2) 0.003(2)
C5' 0.022(3) 0.025(3) 0.018(3) 0.005(3) 0.007(2) 0.005(2)
O5' 0.029(2) 0.026(2) 0.019(2) -0.0026(16) 0.0103(16) -0.0044(17)
C5B 0.028(3) 0.021(3) 0.022(3) 0.004(2) 0.015(3) -0.001(2)
C5G1 0.039(3) 0.021(3) 0.024(3) -0.002(3) 0.019(3) -0.001(2)
C5G2 0.026(3) 0.030(3) 0.040(4) -0.006(3) 0.015(3) 0.006(3)
C5D 0.034(3) 0.031(3) 0.028(3) -0.002(3) 0.012(3) -0.002(3)
O5" 0.048(2) 0.025(2) 0.018(2) -0.0001(17) 0.0171(18) -0.0010(17)
O1W 0.040(3) 0.029(3) 0.031(2) -0.0002(19) 0.016(2) 0.001(2)
O2W 0.039(2) 0.028(3) 0.028(3) -0.004(2) 0.010(2) 0.003(2)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
N1 C1A 1.493(5) . ?
C1A C1' 1.516(7) . ?
C1A C1B 1.524(6) . ?
C1' O1' 1.215(5) . ?
C1' N2 1.331(6) . ?
C1B C1G 1.519(7) . ?
C1G C1D1 1.377(7) . ?
C1G C1D2 1.401(7) . ?
C1D1 C1E1 1.399(6) . ?
C1D2 C1E2 1.398(6) . ?
C1E1 C1Z 1.373(7) . ?
C1E2 C1Z 1.373(7) . ?
N2 C2A 1.450(6) . ?
C2A C2' 1.491(6) . ?
C2' O2' 1.238(5) . ?
C2' N3 1.342(5) . ?
N3 C3A 1.458(6) . ?
C3A C3' 1.508(6) . ?
C3A C3B 1.525(6) . ?
C3' O3' 1.224(5) . ?
C3' N4 1.338(6) . ?
N4 C4A 1.429(6) . ?
C4A C4B 1.317(6) . ?
C4A C4' 1.509(6) . ?
C4' O4' 1.237(5) . ?
C4' N5 1.337(6) . ?
C4B C4G 1.481(6) . ?
C4G C4D1 1.386(7) . ?
C4G C4D2 1.395(6) . ?
C4D1 C4E1 1.383(6) . ?
C4D2 C4E2 1.376(7) . ?
C4E1 C4Z 1.368(7) . ?
C4E2 C4Z 1.368(7) . ?
N5 C5A 1.475(5) . ?
C5A C5B 1.530(6) . ?
C5A C5' 1.539(7) . ?
C5' O5' 1.251(5) . ?
C5' O5" 1.261(5) . ?
C5B C5G1 1.523(6) . ?
C5B C5G2 1.535(6) . ?
C5G1 C5D 1.523(6) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1A C1' 107.2(4) . . ?
N1 C1A C1B 107.6(4) . . ?
C1' C1A C1B 113.1(4) . . ?
O1' C1' N2 123.0(5) . . ?
O1' C1' C1A 120.6(4) . . ?
N2 C1' C1A 116.5(4) . . ?
C1G C1B C1A 114.6(4) . . ?
C1D1 C1G C1D2 118.5(5) . . ?
C1D1 C1G C1B 124.2(5) . . ?
C1D2 C1G C1B 117.3(5) . . ?
C1G C1D1 C1E1 120.6(5) . . ?
C1E2 C1D2 C1G 120.4(5) . . ?
C1Z C1E1 C1D1 120.3(5) . . ?
C1Z C1E2 C1D2 120.0(5) . . ?
C1E1 C1Z C1E2 120.1(5) . . ?
C1' N2 C2A 120.9(4) . . ?
N2 C2A C2' 116.7(4) . . ?
O2' C2' N3 120.9(4) . . ?
O2' C2' C2A 118.9(4) . . ?
N3 C2' C2A 120.2(4) . . ?
C2' N3 C3A 117.4(4) . . ?
N3 C3A C3' 112.4(4) . . ?
N3 C3A C3B 110.6(4) . . ?
C3' C3A C3B 111.1(4) . . ?
O3' C3' N4 121.4(5) . . ?
O3' C3' C3A 121.0(4) . . ?
N4 C3' C3A 117.6(4) . . ?
C3' N4 C4A 122.8(4) . . ?
C4B C4A N4 124.9(4) . . ?
C4B C4A C4' 118.6(4) . . ?
N4 C4A C4' 116.5(4) . . ?
O4' C4' N5 121.3(4) . . ?
O4' C4' C4A 121.5(4) . . ?
N5 C4' C4A 117.3(4) . . ?
C4A C4B C4G 129.1(5) . . ?
C4D1 C4G C4D2 118.2(4) . . ?
C4D1 C4G C4B 123.2(5) . . ?
C4D2 C4G C4B 118.6(4) . . ?
C4E1 C4D1 C4G 120.1(5) . . ?
C4E2 C4D2 C4G 121.0(5) . . ?
C4Z C4E1 C4D1 120.7(5) . . ?
C4Z C4E2 C4D2 119.8(5) . . ?
C4E1 C4Z C4E2 120.2(5) . . ?
C4' N5 C5A 118.7(4) . . ?
N5 C5A C5B 109.9(4) . . ?
N5 C5A C5' 110.9(4) . . ?
C5B C5A C5' 110.9(4) . . ?
O5' C5' O5" 124.6(4) . . ?
O5' C5' C5A 118.8(4) . . ?
O5" C5' C5A 116.4(4) . . ?
C5G1 C5B C5A 111.2(4) . . ?
C5G1 C5B C5G2 111.3(4) . . ?
C5A C5B C5G2 110.0(4) . . ?
C5D C5G1 C5B 114.5(4) . . ?
_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        24.51
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.210
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.053